CN109180440B - Extraction catalytic reaction tower - Google Patents
Extraction catalytic reaction tower Download PDFInfo
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- CN109180440B CN109180440B CN201811323215.1A CN201811323215A CN109180440B CN 109180440 B CN109180440 B CN 109180440B CN 201811323215 A CN201811323215 A CN 201811323215A CN 109180440 B CN109180440 B CN 109180440B
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- reaction tower
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- tube
- catalyst
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- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 38
- 238000000605 extraction Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 72
- 230000018044 dehydration Effects 0.000 claims abstract description 37
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 37
- 239000012528 membrane Substances 0.000 claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 31
- 238000012856 packing Methods 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000006260 foam Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims description 41
- 238000010992 reflux Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910001220 stainless steel Inorganic materials 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 14
- 230000003197 catalytic effect Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 239000003566 sealing material Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 229910010293 ceramic material Inorganic materials 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000000712 assembly Effects 0.000 claims description 4
- 238000000429 assembly Methods 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 18
- 238000006116 polymerization reaction Methods 0.000 abstract description 10
- 239000000047 product Substances 0.000 description 42
- 239000007789 gas Substances 0.000 description 36
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 34
- 239000012071 phase Substances 0.000 description 27
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 21
- 230000002194 synthesizing effect Effects 0.000 description 10
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 238000005194 fractionation Methods 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 230000001174 ascending effect Effects 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000008098 formaldehyde solution Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 230000002745 absorbent Effects 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000003491 array Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000006262 metallic foam Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003204 osmotic effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002844 continuous effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- MGJURKDLIJVDEO-UHFFFAOYSA-N formaldehyde;hydrate Chemical compound O.O=C MGJURKDLIJVDEO-UHFFFAOYSA-N 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- DSMZRNNAYQIMOM-UHFFFAOYSA-N iron molybdenum Chemical compound [Fe].[Fe].[Mo] DSMZRNNAYQIMOM-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000409 membrane extraction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0415—Solvent extraction of solutions which are liquid in combination with membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
- B01J8/009—Membranes, e.g. feeding or removing reactants or products to or from the catalyst bed through a membrane
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
- B01J8/0446—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the flow within the beds being predominantly vertical
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D323/00—Heterocyclic compounds containing more than two oxygen atoms as the only ring hetero atoms
- C07D323/04—Six-membered rings
- C07D323/06—Trioxane
Abstract
An extraction catalytic reaction tower, comprising a reaction tower, wherein the reaction tower internals comprise: a demister, a distributor and a filler assembly; the uppermost end in the reaction tower is provided with a foam remover and a distributor below the foam remover; the distributor is filled with a plurality of sections of filler components, and redistributors are arranged among the sections of filler components; the filler component is communicated with the adjacent distributor and the redistributor; the packing component is a multifunctional membrane component or a multifunctional module component; the top of the reaction tower is provided with a gas phase outlet, the bottom of the reaction tower is provided with a discharge hole, the side wall of the bottom of the reaction tower is provided with a feed inlet, the lowest filler component is provided with a dehydration outlet on the side wall of the reaction tower, and the uppermost distributor of the reaction tower is communicated with a first backflow liquid inlet arranged on the side wall of the reaction tower. The invention can solve the technical problems that the traditional equipment has complex process, long time and low efficiency in the application process, and can not realize the dehydration, polymerization and catalysis processes at one time.
Description
Technical Field
The invention relates to the field of catalytic reaction equipment in the fine chemical industry, in particular to an extraction catalytic reaction tower.
Background
DMMn products are world-recognized environment-friendly oil additives, but the production method is quite complex, trioxymethylene, methylal, dimethyl ether and the like are required to be produced firstly, and the technologies of concentration, extraction, rectification, drying and the like are also utilized to obtain purer raw materials or semi-finished products, so that qualified DMMn finished products can be finally obtained. The traditional equipment has complex process, long time and low efficiency in the application process, so that a reaction device capable of efficiently dehydrating, polymerizing and catalyzing is urgently needed.
Disclosure of Invention
In order to overcome the defects and shortcomings of the technology, the invention provides an extraction catalytic reaction tower, which solves the technical problems that the technology is complex, the time is long, the efficiency is low, and the dehydration, polymerization and catalysis processes can not be realized at one time in the application process of traditional equipment.
The invention adopts the following technical scheme:
an extraction catalytic reaction column comprising a reaction column, the reaction column internals comprising: a demister, a distributor and a filler assembly; the uppermost end in the reaction tower is provided with a foam remover and a distributor below the foam remover; a plurality of sections of filler components are filled under the distributor, and a redistributor is arranged between each section of filler components; the filler assembly is communicated with the adjacent distributor and the redistributor;
the packing component is a multifunctional membrane component or a multifunctional module component;
the multifunctional membrane component or the multifunctional module component comprises a plurality of vertically arranged up-and-down through tubes which are arranged into a tube bed and fixed by a tube plate, a plurality of small holes are formed in the whole body of the tube, the fired up-and-down through functional tubes are inserted into the tube, the inner surfaces of the functional tubes are compositely fired to form the functional membrane, and the functional tubes are filled with fillers;
sealing materials are arranged at the upper end and the lower end of a gap between the tube array and the functional tube for sealing and fixing; the filler component is communicated with the adjacent distributor and the redistributor through the functional pipe to form a reaction channel; a dehydration runner is formed among the filler component, the redistributor and the side wall of the reaction tower;
the top of the reaction tower is provided with a gas phase outlet, the bottom of the reaction tower is provided with a discharge port, the side wall of the bottom of the reaction tower is provided with a feed inlet, the lowest filler component is provided with a dehydration water outlet on the side wall of the reaction tower, and the uppermost distributor of the reaction tower is communicated with a first backflow liquid inlet arranged on the side wall of the reaction tower;
the tube plates at the bottom layer are closed water receiving plates, all the tube plates above the bottom layer are communicated through downcomers, a vacuumizing port is arranged on the tube plate at the highest layer and is connected with an external vacuumizing system, and all the spaces outside the tube arrays of each section, which are communicated by the downcomers, are vacuumized to form negative pressure.
The redistributor positioned in the middle of the reaction tower is communicated with a second reflux liquid inlet arranged on the side wall of the reaction tower.
Diameter of the small hole1-50mm.
The functional pipe is made of ceramic materials through sintering; the functional membrane is prepared by composite firing of any one of ceramic materials, diatomite materials, ZSM-5, SAPO-34 or zeolite molecular sieves and the inner surface of the functional tube.
The packing filled in the multifunctional membrane component is a cylindrical stainless steel corrugated wire mesh structured packing.
The foam remover, the distributor and the redistributor are all internally formed by stainless steel corrugated wire meshes; the distributor and the redistributor are respectively provided with a plurality of diversion ports communicated with the functional pipe.
The filler filled in the multifunctional module assembly is a catalyst module; the module catalyst comprises a catalyst, a wire mesh and a wire mesh corrugated plate, wherein the module catalyst is formed by arranging the wire mesh and the wire mesh corrugated plate in parallel at intervals, catalyst particles are held between two wire mesh plates to form a catalyst layer, and the catalyst particles in the catalyst layer are separated by the wire mesh corrugated plate; the catalyst layers in the module catalyst are arranged at intervals.
The foam remover and the redistributor are formed by arranging stainless steel corrugated wire meshes, and the redistributors are provided with a plurality of flow guide openings communicated with the functional pipes; the distributor is made of stainless steel plates and is provided with a plurality of diversion openings communicated with the functional pipes.
The sealing material is a polytetrafluoroethylene sealing gasket or a metal winding gasket, and an anti-corrosion rubber gasket.
The invention has the following positive and beneficial effects:
the extraction catalytic reaction tower can realize the dehydration, polymerization and catalysis processes in a single device at one time, greatly shortens the process time, reduces the process complexity, and has remarkable effect when synthesizing DMMn products.
Drawings
FIG. 1 is a reaction scheme of an apparatus for synthesizing trioxymethylene and DMMn with a multifunctional membrane;
FIG. 2 is a schematic structural view of the catalytic reaction column of FIG. 1;
FIG. 3 is a schematic cross-sectional structural view of the packing assembly of the catalytic reaction column of FIG. 2;
FIG. 4 is a schematic view showing a longitudinal section of a single tube array in the catalytic reaction column of FIG. 2;
FIG. 5 is a schematic view of a tube array functional tube thickness section structure of a tubular functional membrane module;
FIG. 6 is a reaction scheme of an apparatus for synthesizing DMMn in a one-step process;
FIG. 7 is a schematic view of the catalytic reaction column of FIG. 6;
FIG. 8 is a schematic cross-sectional structural view of the packing assembly of the catalytic reaction column of FIG. 7;
FIG. 9 is a schematic cross-sectional structure of a modular catalyst;
fig. 10 is a schematic view of the structure of a longitudinal section of the catalytic reaction column.
Figure number: 1-methylal oxidation reactor, 2-reaction tower, 211-first reflux inlet, 212-gas phase outlet, 213-inlet, 214-outlet, 215-dewatering outlet, 216-second reflux inlet, 23-packing assembly, 25-multifunctional membrane assembly, 251-column, 252-small hole, 253-functional tube, 254-packing, 255-functional membrane, 26-redistributor, 27-tube sheet, 28-distributor, 29-multifunctional module assembly, 4-fractionation tower, 5-waste heat boiler, 6-heat exchanger, 7-condenser, 8-condensing tank, 9-reflux pump, 10-reboiler, 12-multistage fixed bed reaction tower, 13-finished product fractionation tower, 14-mixer, 15-finished product fractionation tower condenser, 16-finished product fractionation tower reflux tank, 17-finished product fractionation tower reflux pump, 18-multistage fixed bed reaction tower reboiler, 19-finished product fractionation tower reboiler, 20-remover, 31-aqueous formaldehyde solution evaporator, 32-reflux tank, 40-403-catalyst layer, corrugated plate, metal foam layer, 401-down pipe, and 50-metal foam layer.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings.
The following examples are given for the purpose of illustration only and are not intended to limit the embodiments of the invention. Various other changes and modifications may be made by one of ordinary skill in the art in light of the following description, and such obvious changes and modifications are contemplated as falling within the spirit of the present invention.
Referring to the drawings, an extraction catalytic reaction tower comprises a reaction tower 2, wherein the internal components of the reaction tower 2 comprise: a demister 20, a distributor 28, a packing assembly 23; the uppermost end in the reaction tower 21 is provided with a foam remover 20 and a distributor 28 below the foam remover; the distributor 28 is filled with a plurality of sections of filler assemblies 23, and a redistributor 26 is arranged between each section of filler assemblies 23; the filler assembly 23 is communicated with the adjacent distributor 28 and the redistributor 26;
the packing assembly 23 is a multifunctional membrane assembly 25 or a multifunctional module assembly 29;
referring to fig. 2, 3, 4, and 5, the multifunctional membrane module 25 or the multifunctional module 29 includes a plurality of vertically arranged tubes 251 that are vertically penetrated, and arranged in a manner that a tube bed is fixed by a tube plate 27, a plurality of small holes 252 are formed around the tubes 251, a sintered functional tube 253 that is vertically penetrated is inserted into the tubes 251, a functional membrane 255 that is formed by composite firing is formed on the inner surface of the functional tube 253, and a filler 254 is filled in the functional tube 253;
sealing materials are arranged at the upper end and the lower end of a gap between the tube array 251 and the functional tube 253 for sealing and fixing; the packing assembly 23 is communicated with the adjacent distributor 28 and the redistributor 26 through the functional pipe 253 to form a reaction channel; the filler assembly 23, the redistributors 26 and the side wall of the reaction tower 2 form a dehydration runner;
referring to fig. 1 and 6, the top of the reaction tower 2 is provided with a gas phase outlet 212, the bottom is provided with a discharge outlet 214, the side wall of the bottom of the reaction tower 2 is provided with a feed inlet 213, the lowest filler component 23 is provided with a dehydration outlet 215 on the side wall of the reaction tower 2, and the uppermost distributor of the reaction tower 2 is communicated with a first reflux liquid inlet 211 arranged on the side wall of the reaction tower 2;
the bottom layer of tube plates 27 are closed water receiving plates, the tube plates 27 above the bottom layer are communicated through the downcomers 50, the top layer of tube plates 27 are provided with vacuumizing ports and are connected with an external vacuumizing system, and all the spaces outside the tube arrays 251 and communicated by the downcomers 50 are vacuumized.
The redistributor 26 positioned in the middle of the reaction tower 2 is communicated with a second reflux inlet 216 arranged on the side wall of the reaction tower.
Diameter of the small hole 2521-50mm.
The functional pipe 253 is made of ceramic materials through sintering; the functional membrane 255 is made by composite firing of any one of ceramic material, diatomite material, ZSM-5, SAPO-34 or zeolite molecular sieve and the inner surface of the functional tube 253.
The packing 254 filled in the multifunctional membrane module 25 is a structured packing of a stainless steel corrugated wire mesh in a cylindrical shape.
The foam remover 20, the distributor 28 and the redistributor 26 are all internally composed of stainless steel corrugated wire meshes; the distributor 28 and the redistributor 26 are respectively provided with a plurality of flow guiding ports communicated with the functional pipes 253.
Referring to fig. 7, 8, 9, the packing 254 filled in the multi-function module assembly 29 is a catalyst module 40; the module catalyst 40 comprises a catalyst, a wire mesh 402 and a wire mesh corrugated plate 403, wherein the module catalyst 40 is formed by arranging the wire mesh 402 and the wire mesh corrugated plate 403 in parallel at intervals, the catalyst particles are held between two wire mesh 402 to form a catalyst layer 401, and the catalyst particles in the catalyst layer 401 are separated by the wire mesh corrugated plate 403; the catalyst layers 401 in the module catalyst 40 are disposed at intervals.
The foam remover 20 and the redistributor 26 are formed by arranging stainless steel corrugated wire meshes, and the redistributors 26 are provided with a plurality of flow guide ports communicated with the functional pipes 253; the distributor 28 is made of stainless steel plate and is provided with a plurality of flow guiding ports communicated with the functional pipe 253.
The sealing material is a polytetrafluoroethylene sealing gasket or a metal winding gasket, and an anti-corrosion rubber gasket.
Sealing materials are arranged at the upper end and the lower end of a gap between the tube array 251 and the functional tube 253 for sealing and fixing, and the sealing materials are polytetrafluoroethylene sealing gaskets or metal winding gaskets and anti-corrosion rubber gaskets; the sealing material may be fastened and fixed by using a bolt fastener in the present invention.
The working principle of the invention is as follows:
the inside of the tube array 251 is communicated with the distributor 28 and the redistributor 26 to form vertical gas phase and extraction channels, and a water channel is formed between the outside of the tube array 251 and the inner wall of the reaction tower 2.
After entering from the first reflux inlet 211 at the top of the column, the extract flows into the column 251 of the packing assembly 23 via the distributor 28, and is dispersed by the packing 254 in the column 251.
After the oxidizing gas enters through the feed inlet 213 at the bottom of the tower, the oxidizing gas enters the tube array 251 through the lowest redistributor 26 to rise, the oxidizing gas is extracted by the extraction liquid in the filler 254 in the functional membrane 255 and is dehydrated with the functional membrane 255, water seeps out from the tube array 251 from the small holes 252 due to osmotic pressure, the oxidizing gas is gathered downwards on the lowest tube plate 27 and flows out through the dehydration water outlet 215, and unreacted gas continues to rise and react repeatedly; water from the upper reaction flows from the leaked tube plate 27 to the bottom-most closed tube plate 27; the gas is extracted and dehydrated for multiple times, and is refined again by the demister 20 at the top of the tower and then discharged from the gas phase outlet 212. The reacted extract phase is discharged from the discharge port 214.
Application example one
The device is applied to a method for synthesizing trioxymethylene and DMMn by using a multifunctional membrane:
firstly, methylal raw materials and air are heated and mixed and enter a methylal oxidation reactor 1, oxidation reaction is carried out under the action of an iron-molybdenum catalyst, oxidation products are generated, the oxidation products are discharged and then are subjected to heat exchange through a heat exchanger 6, the oxidation products are introduced into a feed inlet 213 of a multifunctional membrane extraction dehydration catalytic reaction tower 2, the materials enter the extraction dehydration catalytic reaction tower 2 through a built-in redistributor 26 to undergo physical catalytic chemical reaction, under the extraction action of an extractant entering through a first reflux feed inlet 211, the generated and dehydrated extraction phase of trioxymethylene is discharged through a discharge port 214, residual gas continues to ascend to a gas phase outlet 212 of the reaction tower in the tower, part of the residual gas is processed and exhausted, and the other part of the residual gas returns to the methylal oxidation reactor 1 for recycling.
Step two, the trioxymethylene extract phase generated by the extraction dehydration catalytic reaction tower 2 and discharged by the discharge port 214 is led into the inlet of the fractionating tower 4, and the extract phase is led into a condenser 7, a condensing tank 8 and a reflux pump 9 through the outlet under the heating action of a reboiler 10 of the fractionating tower 4, wherein the gas phase (extractant) is divided into two paths: one path of the waste water flows back into the fractionating tower 4, the other path of the waste water returns to the liquid inlet 211 of the extraction dehydration catalytic reaction tower 2 for recycling, and the outlet at the bottom of the fractionating tower 4 is discharged to obtain a refined high-purity trioxymethylene intermediate product.
And step three, fully mixing the high-purity trioxymethylene obtained in the step two with high-purity methylal in a certain proportion in a mixer 14, introducing the mixture into a multi-stage fixed bed reaction tower 12, carrying out continuous polymerization chemical reaction under the action of a resin catalyst to produce a DMMn primary product, and fractionating the DMMn primary product by a finished product fractionating tower 13 to obtain a DMM3-6 final product. The gas phase in the finished product fractionating tower 13 is discharged and then flows back into the multi-stage fixed bed reaction tower 12 through a condenser 15 of the finished product fractionating tower, a reflux tank 16 of the finished product fractionating tower and a reflux pump 17 of the finished product fractionating tower.
The method for synthesizing trioxymethylene and DMMn by using the multifunctional membrane generally comprises the following steps:
(1) Oxidizing reaction;
(2) Polymerization reaction;
(3) Extracting reaction;
(4) Fractionating;
(5) DMMn was synthesized.
When the catalyst is applied to the polymerization and extraction reactions in the steps (2) and (3), the multifunctional membrane module 25 integrating dehydration and catalysis is filled in the catalytic reaction tower 2 (CTC tower), the module is formed by sintering a functional membrane 255 and a functional tube 253 into a geometric body such as a steel tube, and inserting the geometric body into the tube 253 made of a supporting material, the functional membrane 255 is made of a material with the function of catalyzing and synthesizing trioxymethylene, in particular ceramics, diatomite, ZSM-5, SAPO-34, zeolite molecular sieve and the like, wherein after the ZSM-5, SAPO-34 and zeolite molecular sieve are made into the functional membrane, the module not only has the dehydration function, but also has the high catalytic function, and the structure and the shape are shown in figures 3, 4 and 5; the functional membrane 255 in the first embodiment is made of ZSM-5, and has a molecular pore of 1-5×10 -1 nm, the functional tube 253 is fired from ceramic 75 into a ceramic tube, wherein Al 2 O 3 The content is controlled to be more than 75%, the rest components are conventional, and the ceramic 75 is an existing material and can be purchased from outside; the tube array is a metal tube. The catalytic reaction tower 2 is composed of tower internals and a multifunctional membrane module 25, wherein the tower internals comprise: demister 20, redistributor 26, packing assembly 23, and tube sheet 27 holding multifunctional membrane assembly 25. The multifunctional membrane module 25 is arranged like a tube bed, the functional tubes 253 are inserted into the tubes 251, and the tubes 251 are opened with diameters around the whole bodyA plurality of small holes 252 to facilitate the water to be removed to leave the material system in time and be discharged; the tube array 251 and the functional tube 253 are sealed and fixed by sealing materials such as sealing gaskets, the materials are not mutually communicated, and the pressure on the inner side and the outer side of the functional tube 253The pressure inside is unequal, and osmotic pressure exists relative to the outside, so that the dehydrated water can be easily oozed out of the functional pipe 253 and discharged through the small holes 252 on the row pipe 251. The packing assembly 23 in the tower is filled in sections, the filling amount is N sections, N is less than or equal to 1 and less than or equal to 100, and the height of each section is 1-3m; each section of filling functional pipe 253 is M, and M is more than or equal to 1 and less than or equal to 5000; each pipe diameter is D, D is less than or equal to 5 and less than or equal to 200cm, a redistributor 26 is arranged between each two sections, and a foam remover 20 is arranged on a first reflux liquid inlet 211 at the upper part of the tower, namely an extractant inlet and is used for recycling the extractant which is led to a gas phase outlet 212; the body of each functional pipe 253 is filled with a stainless steel corrugated wire mesh structured packing such as a cylindrical geometry.
Application example II
The device is applied to a method for synthesizing DMMn by a one-step method:
in the first step, a 5-99% aqueous formaldehyde solution is first vaporized in an aqueous formaldehyde solution evaporator 31.
Step two, dehydration, polymerization and synthesis, and physical and chemical reactions occur simultaneously: the gas phase material produced in the first step introduced from the inlet 213 of the catalytic reaction tower 2 is first introduced into the tube side of the functional tube 253 of the multifunctional module assembly 29 by the lower distributor, and undergoes polymerization reaction under the synergistic effect of catalytic dehydration of the packing assembly 23 in the tower to generate an aqueous trioxymethylene solution, and then as the gas flow continues to go upward, is dehydrated while being respectively absorbed by methylal (hereinafter abbreviated as M1) and polydimethoxydimethyl ether (hereinafter abbreviated as M2) which are respectively added from the second reflux inlet 216 and the first reflux inlet 211 and distributed by the middle distributor and the upper distributor 28, and continuously undergoes chemical reaction for synthesizing DMMn under the continuous effect of the module catalyst 40 of the multifunctional module assembly 29, and gradually goes downward to finally fall into the bottom of the tower due to the high DMMn density, but simultaneously under the function of dehydration of the functional film, the dehydrated water is continuously discharged from the dehydration and water discharge outlet 215, the concentration of formaldehyde and trioxymethylene in the downstream flow of air is higher and lower, and the formaldehyde and trioxymethylene in the upstream flow of air continuously transfer mass and heat with the oncoming absorbents, namely M1 and M2, when the air goes up to the adjacent redistributor 26, the air goes up to the tube side of the functional tube 253 of the adjacent second-stage multifunctional module assembly 29, and the physicochemical reaction, namely the water in the formaldehyde removing aqueous solution, is carried out again, the formaldehyde is polymerized into trioxymethylene, the DMMn is synthesized, so the cycle is repeated until the formaldehyde and the trioxymethylene in the gas phase component are thoroughly reacted, after the residual gas phase in the reaction goes up to the foam remover 20, the trioxymethylene in mist entrainment is removed completely, and the gas phase component is discharged from the gas phase outlet 212, the main component is methylal M1, then sequentially passing through the condenser 7, the reflux tank 32 and the reflux pump 9, and then refluxing to the second liquid inlet 216 for continuous reaction and recycling; the DMMn product is discharged from the discharge port 214 of the tower and is led into the finished product fractionating tower 13, and the dehydrated water, namely the water in the formaldehyde water solution, is discharged from the tower through the dehydration port 215 under the dual functions of negative pressure and dehydration of the functional film in the shell side of the dehydration catalytic reaction tower 2.
Step three, fractionating a finished product: referring to fig. 6, after the DMMn primary product obtained in the second step is introduced into the finished product fractionating tower 13 from the inlet of the finished product fractionating tower 13, fractionation is performed in a heated state of the reboiler 10 of the finished product fractionating tower, so as to obtain a gas phase and a liquid phase; the gas phase is absorbent M2, the gas phase is discharged through a gas outlet and enters a condenser 15 of a finished product fractionating tower for condensation, the liquid M2 obtained after condensation sequentially flows through a reflux tank 16 of the finished product fractionating tower and a reflux pump 17 of the finished product fractionating tower and is divided into two paths, one path of liquid M2 flows back into the finished product fractionating tower 13, and the other path of liquid M2 returns into the dehydration catalytic reaction tower 2 for recycling; the bottom liquid phase of the finished product fractionating tower 13 is a high-purity DMMn finished product, and is discharged from a discharge port and collected by a finished product tank.
The reaction steps of a device for synthesizing DMMn by a one-step method can be summarized as follows:
(1) Vaporizing the formaldehyde aqueous solution;
(2) Dehydration, polymerization, synthesis, and physicochemical reactions occur simultaneously;
(3) And (3) fractional distillation reaction.
The working process of the catalytic reaction tower 2 in the reaction for synthesizing DMMn by a one-step method is as follows: firstly, the gas obtained in the step (1) enters from the feed inlet 213 and enters the tube side of the functional tube 253 in the multifunctional module assembly 29, and in the second embodiment, the functional film 255 is made of Z materialSM-5, the formed intramolecular pore diameter is 2-3x10 -1 nm, the functional tube 253 is fired from ceramic 75 into a ceramic tube, wherein Al 2 O 3 The content is 75%, the rest components are conventional, and the ceramic 75 is the existing material and can be purchased from outsourcing; the tube array is a metal tube. The catalyst particles in the catalyst module 40 in the multifunctional module assembly 29 are D006 resin catalysts, under the synergistic effect of the catalytic function and the dehydration function of the filler assembly 23 in the catalytic reaction tower 2, polymerization reaction is carried out to generate trioxymethylene aqueous solution, then the trioxymethylene aqueous solution is gradually extracted by an oncoming extractant and falls into the tower bottom along with the continuous ascending of oxidizing gas flow, but simultaneously under the effect of the dehydration function of the filler assembly 23, the concentration of trioxymethylene in the ascending oxidizing gas flow is higher and lower, and the ascending of the trioxymethylene aqueous solution and unreacted formaldehyde component in the oncoming extractant transfer heat and mass when reaching the adjacent redistributor 26, the ascending of the trioxymethylene aqueous solution is continued to enter the tube pass of the adjacent second-stage filler assembly 23, so that the physicochemical reaction is continued, the cycle is repeated until the formaldehyde in the oxidizing component is thoroughly reacted, and the residual reaction gas is continuously ascended in the tower to the demister 20, and the extracting agent entrained by mist is removed completely, and the mist is discharged from the gas phase outlet 212; the extract phase of the trioxymethylene enters the finished product fractionating tower 13 through the discharge port 214 of the catalytic reaction tower 2, and the dehydrated water is discharged out of the tower through the dehydration port 215 under the double functions of negative pressure and dehydration of the functional film in the shell side.
The dehydration catalytic reaction tower 2 is designed as follows: a multi-function module assembly 29 having a loading of 3 segments, each segment having a height of 1m; 5 filling functional pipes 253 are arranged in each section; each pipe diameter is 5cm, a redistributor 26 is arranged between each two sections, a foam remover 20 is arranged on a first backflow liquid inlet 211 at the uppermost end of the tower, namely an extractant inlet, and a catalyst 40 like a patent CN211621189748.5 module is arranged in each functional pipe 253; the demister 20 and the redistributor 26 are made of stainless steel corrugated wire mesh.
The operating conditions of the dehydration catalytic reaction column 2 were designed as follows:
the catalytic operating conditions were: the temperature of the tower top is 70-90 ℃, 0.1MPa, the temperature of the tower bottom is 80-100 ℃, 0.2MPa, 228g of methylal (three times mole of formaldehyde) is added from a 2E port;
the dehydration operation conditions are as follows: the outside of the functional pipe 253 is sleeved with a tube array 251, and the whole body is provided with a diameterA plurality of small holes 252, which facilitate the timely drainage of the water removed out of the system, and control the operating pressure as follows: -0.03Mpa; water from which 40g of the aqueous formaldehyde solution was removed is discharged from the dehydration port 215;
DMMn is synthesized, under the action of a module catalyst 40, 1 mole of formaldehyde and 1 mole of methylal generate 106.0g of polydimethoxy dimethyl ether (M2), the polydimethoxy dimethyl ether is discharged from a discharge port 214 and is introduced into a finished product fractionating tower 13, and the gas phase is distilled and enters a dehydration catalytic reaction tower 2 again through a first reflux liquid inlet 211 for continuous reaction through a condenser 7 and a reflux pump 9.
After the DMMn primary product obtained in the second step enters a finished product fractionating tower 13, fractionating the DMMn primary product in a heating state of a reboiler 10 of the finished product fractionating tower 13 to obtain a gas phase and a liquid phase; the gas phase is absorbent M2, the gas phase is discharged through an exhaust port and enters a condenser 7 for condensation, the liquid M2 obtained after condensation sequentially flows through a reflux tank 32 and a reflux pump 9 and is divided into two paths, one path flows back to a finished product fractionating tower 13, and the other path returns to the dehydration catalytic reaction tower 2 for recycling through a first reflux inlet 211 of the dehydration catalytic reaction tower 2; the liquid phase at the bottom outlet of the finished product fractionating tower 13 is a high-purity DMMn finished product, and is discharged from a discharge outlet and collected by a finished product tank.
Claims (8)
1. Extraction catalytic reaction tower, including reaction tower (2), reaction tower (2) internals include: a demister (20), a distributor (28) and a filler assembly (23); the device is characterized in that a demister (20) is arranged at the uppermost end in the reaction tower (2), and a distributor (28) is arranged below the demister; the distributor (28) is filled with a plurality of sections of filler assemblies (23) downwards, and a redistributor (26) is arranged between each section of filler assemblies (23); -said filler assembly (23) communicating with adjacent said distributor (28), said redistributor (26);
the packing assembly (23) is a multifunctional membrane assembly (25) or a multifunctional module assembly (29);
the multifunctional membrane assembly (25) or the multifunctional module assembly (29) comprises a plurality of vertically arranged up-and-down through tubes (251) which are arranged in a tube bed and fixed by a tube plate (27), a plurality of small holes (252) are formed in the whole body of each tube (251), the sintered up-and-down through functional tubes (253) are inserted into the tubes (251), functional membranes (255) are formed by composite firing of the inner surfaces of the functional tubes (253), and fillers (254) are filled in the functional tubes (253);
sealing materials are arranged at the upper end and the lower end of a gap between the tube array (251) and the functional tube (253) for sealing and fixing; the packing assembly (23) is communicated with the adjacent distributor (28) and the redistributors (26) through the functional pipes (253) to form a reaction channel; a dehydration runner is formed among the filler component (23), the redistributor (26) and the side wall of the reaction tower (2);
the top of the reaction tower (2) is provided with a gas phase outlet (212), the bottom of the reaction tower is provided with a discharge port (214), the side wall of the bottom of the reaction tower (2) is provided with a feed port (213), the lowest filler component (23) is provided with a dehydration water outlet (215) on the side wall of the reaction tower (2), and the uppermost distributor of the reaction tower (2) is communicated with a first backflow liquid inlet (211) arranged on the side wall of the reaction tower (2);
the tube plates (27) at the bottommost layer are closed water receiving plates, all the tube plates (27) above the bottom layer are communicated through downcomers (50), a vacuumizing port is formed in the tube plate (27) at the topmost layer and is connected with an external vacuumizing system, and all the spaces outside the tubes (251) at each section and communicated by the downcomers (50) are vacuumized;
the functional pipe (253) is made of ceramic materials through sintering; the functional membrane (255) is prepared by composite firing of any one of ceramic materials, diatomite materials, ZSM-5, SAPO-34 or zeolite molecular sieves and the inner surface of the functional tube (253).
2. The extraction catalytic reactor as claimed in claim 1, characterized in that a redistributor (26) in the middle of the reactor (2) communicates with a second reflux inlet (216) provided in the side wall of the reactor.
3. The extraction catalytic reactor as claimed in claim 1, characterized in that said apertures (252) have a diameter1-50mm.
4. The extraction catalytic reactor as claimed in claim 1, characterized in that said packing (254) packed in said multifunctional membrane module (25) is a cylindrical structured packing of stainless steel corrugated wire mesh.
5. The extraction catalytic reactor as claimed in claim 1, characterized in that the internal parts of said demister (20), distributor (28) and redistributor (26) are all composed of stainless steel corrugated wire mesh; the distributor (28) and the redistributor (26) are respectively provided with a plurality of diversion ports communicated with the functional pipe (253).
6. The extraction catalytic reactor as claimed in claim 1, characterized in that said packing (254) filled in said multifunctional module assembly (29) is a catalyst module (40); the module catalyst (40) comprises a catalyst, a wire mesh (402) and a wire mesh corrugated plate (403), wherein the module catalyst (40) is formed by arranging the wire mesh (402) and the wire mesh corrugated plate (403) in parallel at intervals, a catalyst layer (401) is formed by bearing the catalyst particles between the two wire mesh (402), and the catalyst particles in the catalyst layer (401) are separated by the wire mesh corrugated plate (403); the catalyst layers (401) in the module catalyst (40) are arranged at intervals.
7. The extraction catalytic reaction tower according to claim 6, wherein the foam remover (20) and the redistributor (26) are arranged by stainless steel corrugated wire mesh, and the redistributors (26) are provided with a plurality of flow guiding ports communicated with the functional pipe (253); the distributor (28) is made of stainless steel plates and is provided with a plurality of flow guide openings communicated with the functional pipes (253).
8. The extraction catalytic reactor as claimed in claim 1, wherein the sealing material is a polytetrafluoroethylene sealing gasket or a metal winding gasket, and an anti-corrosion rubber gasket.
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| CN101480591A (en) * | 2008-01-11 | 2009-07-15 | 山东科技大学 | Tubular reaction fractionating tower |
| CN103801101A (en) * | 2012-11-08 | 2014-05-21 | 邱力 | Despumating type filled tower |
| CN203750547U (en) * | 2014-03-27 | 2014-08-06 | 浙江衢州万能达科技有限公司 | KF catalysis component |
| CN104549057A (en) * | 2015-02-05 | 2015-04-29 | 青岛亿明翔精细化工科技有限公司 | Multipurpose tubular packed reactor |
| CN105622366A (en) * | 2016-03-14 | 2016-06-01 | 凯瑞环保科技股份有限公司 | Device and method for producing polyoxymethylene dimethyl ether DMM3-5 |
| CN105693479A (en) * | 2016-03-15 | 2016-06-22 | 江苏凯茂石化科技有限公司 | Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas |
| CN209242963U (en) * | 2018-11-08 | 2019-08-13 | 凯瑞环保科技股份有限公司 | Extract catalytic tower |
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2018
- 2018-11-08 CN CN201811323215.1A patent/CN109180440B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101480591A (en) * | 2008-01-11 | 2009-07-15 | 山东科技大学 | Tubular reaction fractionating tower |
| CN103801101A (en) * | 2012-11-08 | 2014-05-21 | 邱力 | Despumating type filled tower |
| CN203750547U (en) * | 2014-03-27 | 2014-08-06 | 浙江衢州万能达科技有限公司 | KF catalysis component |
| CN104549057A (en) * | 2015-02-05 | 2015-04-29 | 青岛亿明翔精细化工科技有限公司 | Multipurpose tubular packed reactor |
| CN105622366A (en) * | 2016-03-14 | 2016-06-01 | 凯瑞环保科技股份有限公司 | Device and method for producing polyoxymethylene dimethyl ether DMM3-5 |
| CN105693479A (en) * | 2016-03-15 | 2016-06-22 | 江苏凯茂石化科技有限公司 | Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas |
| CN209242963U (en) * | 2018-11-08 | 2019-08-13 | 凯瑞环保科技股份有限公司 | Extract catalytic tower |
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